CN105731543A - Laser rapid preparation method of inorganic molybdenum disulfide microsphere with fullerene like structure - Google Patents
Laser rapid preparation method of inorganic molybdenum disulfide microsphere with fullerene like structure Download PDFInfo
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- CN105731543A CN105731543A CN201610001020.XA CN201610001020A CN105731543A CN 105731543 A CN105731543 A CN 105731543A CN 201610001020 A CN201610001020 A CN 201610001020A CN 105731543 A CN105731543 A CN 105731543A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/22—Compounds containing sulfur, selenium or tellurium
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/065—Sulfides; Selenides; Tellurides
- C10M2201/066—Molybdenum sulfide
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
Abstract
The invention discloses a laser rapid preparation method of an inorganic molybdenum disulfide microsphere with a fullerene like structure. The preparation method comprises the following steps: dissolving molybdenum disulfide powder into an organic solvent to form suspension liquid; radiating the suspension liquid by pulse laser so as to convert the molybdenum disulfide powder into a fullerene like structure under the effect of the organic solvent and pulse laser; after radiation, subjecting the suspension liquid to centrifugation and separation, and drying the obtained precipitate so as to obtain the inorganic molybdenum disulfide microsphere with a fullerene like structure. Molybdenum disulfide suspension liquid is directly radiated by laser beams, so that molybdenum disulfide powder in suspension liquid can obtain great energy in a very short time (nano second level), molybdenum disulfide powder is ablated and rapidly cooled (nano second level) by the solvent; and molybdenum disulfide microsphere is prepared therefore. The method has the advantages of simple operation, low cost, high product purity, and no impurity. The obtained molybdenum disulfide microsphere can reduce the friction during the friction process.
Description
Technical field
The preparation method that the present invention relates to a kind of mos2 microsphere with similar Fuller olefin structure, it is specifically related to a kind of method that formation adopting pulse laser irradiation simple and quick has the mos2 microsphere of similar Fuller olefin structure, belongs to the preparing technical field of micro-nano powder.
Background technology
Molybdenum bisuphide (the 2H-MoS of layer structure2) as traditional kollag, lubricating oil, grease additive be used widely, but owing to its end exists dangling bonds, chemism is higher, it is easy to oxidized so that coefficient of friction raises, and limits its use in moist and oxygen enriched environment.Within 1993, Margulis proposes inorganic fullerene molybdenum disulfide (IF-MoS first2) preparation method (Nature, 1993,365:113-114), relative to the 2H-MoS of lamellar2Granule, IF-MoS2Having spherical or cylindrical structural, its outer shell is closed, and surface is absent from dangling bonds, has good chemical stability, therefore, and IF-MoS2Remaining to show the tribological property of excellence under harsh working environment, it causes the extensive concern of domestic and international scientist in the potential application of various fields.
At present, IF-MoS2Preparation method mainly has liquid phase method and vapor phase method.Liquid preparation methods technique is loaded down with trivial details, it is necessary to MoS3Or MoO3Nanoparticle is as presoma, and the preparation of presoma is complicated, technique is loaded down with trivial details, need to using high-purity Ar as protective gas in preparation process, and the product impurity obtained is many.Vapor phase method mainly has two classes: one is at H under high temperature2S and high-purity H2Thermally decomposing ammonium thiomolybdate in atmosphere, two is MoO under high temperature3And H2S gas is at H25%+95%N2Reducing atmosphere in there is synthetic reaction, its operating environment requirements is harsh, it is necessary to use hypertoxic gas H expensive, that corrosivity is strong2S, complex process, cost is high.Therefore, more economically, simply, effective IF-MoS2Preparation method, still falls within technological gap.
Summary of the invention
In order to overcome the deficiencies in the prior art, the preparation method that the invention provides a kind of mos2 microsphere with similar Fuller olefin structure, the method is simple to operate, and flow process is short, consuming time few, it is possible to quickly form the mos2 microsphere of similar Fuller olefin structure.
The present invention is directed to the deficiencies such as existing fullerene structured molybdenium disulfide preparation technology is loaded down with trivial details, condition is harsh, propose first to adopt the mode of pulse laser irradiation to prepare fullerene structured molybdenium disulfide.Pulse laser can produce high temperature and high pressure environment at moment (nanosecond order), can rapidly by molybdenum bisuphide ablation, molybdenum bisuphide after ablation cools down rapidly under low temperature organic solvent environment, under the combined effect of pulse laser and low temperature organic solvent, realize the fast transition of molybdenum bisuphide pattern, obtain the molybdenum bisuphide of similar Fuller olefin structure.The method is simple to operate, reaction is quickly, it is to avoid vapor phase method and the deficiency such as liquid phase method conditional is harsh, complex process is loaded down with trivial details, expensive.
The concrete technical scheme of the present invention is as follows:
The preparation method of a kind of mos2 microsphere with similar Fuller olefin structure, is characterized in that comprising the following steps:
(1) molybdenum disulfide powder is disperseed in organic solvent, form suspension；
(2) with the above-mentioned suspension of pulse laser irradiation, molybdenum disulfide powder is made to be changed into similar Fuller olefin structure under the effect of organic solvent and pulse laser；
(3) irradiation complete after, by centrifugal for suspension, separate, gained precipitation is dry, obtains the mos2 microsphere with similar Fuller olefin structure.
Raw material used by the present invention is molybdenum disulfide powder, and the purity of this powder is more than 90%, it is possible to commercially obtain.The microscopic appearance of this molybdenum disulphide powder powder stock is random, for bulk, lamellar, the shape such as bar-shaped admixture.
The inventive method cooperatively forms similar Fuller olefin structure by pulse laser and low-temperature solvent.In selecting organic solvent, first have to select the insoluble solvent also not corroding molybdenum bisuphide, but finding when research, the kind of organic solvent has a certain impact for the formation of fullerene pattern, when the organic solvent selected is suitable, it is easily formed fullerene pattern, and product pattern is single, do not have the molybdenum bisuphide doping of other patterns, and when the molybdenum bisuphide selected is improper, in product except similar Fuller olefin structure, also has the molybdenum bisuphide doping of other patterns.It has been investigated that, adopt and can obtain qualified similar Fuller olefin structure during dimethylformamide.
In step of the present invention (1), molybdenum bisuphide concentration in organic solvent is 0.1～15mg/mL.Molybdenum bisuphide concentration in organic solvent is not easily excessive, and concentration is excessive cannot make all molybdenum bisuphide receive identical energy uniformly in irradiation process, and organic solvent content is very few simultaneously also cannot make the molybdenum bisuphide of ablation quickly cool down.
Further, before in stock dispersion to organic solvent, first raw material being ground, makes powder size at below 1um.Even-grained powder is not only beneficial to dispersion, also make energy that the product unit are that irradiation produces accepts closer to, make product pattern evenly.
In step of the present invention (2), the running parameter of pulse laser is as follows: wavelength is 193nm～1534nm, and frequency is 5～10Hz, and pulse width is 1～50ns, and energy density is 500～1800mJpulse-1cm-2, exposure time is 5～600min.In the specific embodiment of the present invention, pulse laser is formed in the following ways: given off laser beam by laser instrument, then through illuminator and convex lens focus, forms the pulse laser beam of required spot size, adjust to required running parameter, irradiation operations can be carried out.
Preferably, in step (2), the energy density of pulse laser is 1200～1800mJpulse-1cm-2。
Preferably, in step (2), pulse laser irradiation 5-60min can obtain good product.
Further, in order to enable the molybdenum bisuphide of ablation quickly to cool down, in pulse laser irradiation process, it is preferable that the temperature controlling suspension is 0 DEG C～5 DEG C.The modes such as the control ice bath of this low temperature realize.
Further, in order to make irradiation evenly, suspension is stirred pulse laser irradiation, and mixing speed is 100～1500r/min.
In above-mentioned steps (3), that gained precipitation dries in order that abundant volatile organic solvent, the dry mode that can adopt low-temperature heat, heating-up temperature is not above the boiling point of organic solvent, it may be necessary to adopt heating under reduced pressure.
Said method of the present invention can obtain the molybdenum bisuphide of similar Fuller olefin structure, the mos2 microsphere of this structure has the performances such as more excellent antifriction in friction process than common molybdenum disulfide powder, as kollag, lubricating oil, grease anti-friction agent there is better effect, addition is at about 0.15wt%.
Molybdenum disulfide powder is dispersed in liquid flux by the present invention, form suspension, laser beam this suspension of direct irradiation after illuminator and convex lens focus, the molybdenum disulfide powder moment (nanosecond order) in solvent is made to obtain high-energy ablated and by solution rapidly (nanosecond order) cooling, thus realizing the preparation of fullerene molybdenum disulfide microsphere.Compared with prior art, the invention have the benefit that
This preparation method is novel, product purity height free from admixture pollutes, and gained mos2 microsphere has the excellent properties such as antifriction in friction process.
(1) present invention has only to a step and can realize molybdenum disulfide particles from irregular shape to the transformation of inorganic fullerene structure, and simple to operate, preparation cost is low.
(2) present invention may apply to the molybdenum disulfide powder of different primary morphology, as lamellar, bulk, the different-shape such as bar-shaped molybdenum disulfide powder, material choice scope is wide.
(3) preparation process of the present invention has only to the molybdenum disulfide powder that laser irradiation is dispersed in liquid solution, do not need other redox condition, reaction reagent and complex experiment device, condition is easily-controllable, technique is simple, cost is low, solves existing preparation process complexity and is difficult to the difficult problem produced in batches.
(4) product purity that the inventive method obtains is high, free from admixture pollutes, fullerene molybdenum disulfide microsphere has elastic and stronger adsorptivity, as lubricating oil, lubricating oil, grease additive time can be adsorbed onto surface of friction pair, make between metallic rubbing pairs separated from one another, it is effectively reduced friction and wear, there is the excellent properties such as antifriction.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of random molybdenum disulphide powder powder stock；
Fig. 2 is the scanning electron microscope diagram of the molybdenum bisuphide product formed after pulse laser irradiation；
Fig. 3 is the transmission electron microscope figure of the molybdenum bisuphide product formed after pulse laser irradiation；
Fig. 4 is the scanning electron microscope diagram of comparative example 1 products obtained therefrom；
Fig. 5 is the scanning electron microscope diagram of comparative example 2 products obtained therefrom.
Detailed description of the invention
Below embodiments of the invention are elaborated, following embodiment premised on the technology of the present invention under be carried out, give detailed embodiment and concrete operating process, but protection scope of the present invention be not limited to following embodiment.
In following embodiment, described original molybdenum disulphide powder and molybdenum bisuphide raw material, gained directly bought by this raw material from market, or by commercially available prod through grinding gained.
Embodiment 1
(1) weigh the original molybdenum disulphide powder of 750mg (purity 98%, granularity 800nm) in 100mL beaker, add 50mL dimethylformamide, ultrasonic disperse 30min, form suspension；
(2) suspension that will be prepared by krypton fluorine laser bundle (248nm) irradiation above-mentioned steps (1) after illuminator and convex lens focus, the molybdenum disulfide powder in ablation solvent, laser energy density is 1800mJpulse-1cm-1, frequency is 10Hz, and laser pulse is 5ns, and exposure time is 20min.In laser beam irradiation process, the container filling suspension is placed in mixture of ice and water and keeps low temperature, and be stirred continuously suspension with magnetic stirrer with 1500r/min rotating speed.
(3) irradiation complete after, centrifuged suspension, then dried powder at 60 DEG C, obtains product.
Fig. 1 is the scanning electron microscope diagram of original molybdenum disulfide powder in step (1), it can be seen that the pattern of molybdenum bisuphide is various, random in a jumble in raw material.Fig. 2 is the scanning electron microscope diagram of products obtained therefrom after irradiation, it can be seen that product pattern is single, for microsphere, Microsphere Size is comparatively uniform.Fig. 3 is the transmission electron microscope picture of products obtained therefrom after irradiation, as can be seen from the figure the spacing (0.62nm) in microsphere edge (002) face occurs in that the lattice dilatation of 1%, illustrate that marginal portion occurs curling, stress change causes that greatly interlamellar spacing becomes big, occur in that similar Fuller olefin structure, effectively eliminate the dangling bond at grain edges place.So, in friction process, this structure restrained effectively the bad phenomenon that molybdenum disulfide powder makes coefficient of friction raise because high temperature is oxidized.
Embodiment 2
(1) weigh the original molybdenum disulphide powder of 250mg (purity 98%, granularity 600nm) in 100mL beaker, add 50mL dimethylformamide, ultrasonic disperse 20min, form suspension.
(2) suspension that will be prepared by krypton fluorine laser bundle (248nm) irradiation above-mentioned steps (1) after illuminator and convex lens focus, the molybdenum disulfide powder in ablation solvent, laser energy density is 1600mJpulse-1cm-1, frequency is 8Hz, and laser pulse is 25ns, and exposure time is 30min.In laser beam irradiation process, the container filling suspension is placed in mixture of ice and water and keeps low temperature, and be stirred continuously suspension with magnetic stirrer with the rotating speed of 1000r/min.
(3) irradiation complete after, centrifuged suspension, dried powder at 60 DEG C, obtain fullerene molybdenum disulfide microsphere.Products obtained therefrom pattern is similar to Example 1.
Embodiment 3
(1) weigh the original molybdenum disulphide powder of 25mg (purity 98%, granularity 400nm) in 100mL beaker, add 50mL dimethylformamide, ultrasonic disperse 10min, form suspension.
(2) suspension that will be prepared by krypton fluorine laser bundle (248nm) irradiation above-mentioned steps (1) after illuminator and convex lens focus, the molybdenum disulfide powder in ablation solvent, laser energy density 1000mJpulse-1cm-1, frequency 5Hz, laser pulse 50ns, exposure time is 40min.In laser beam irradiation process, the container filling suspension is placed in mixture of ice and water and keeps low temperature, and be stirred continuously suspension with magnetic stirrer with the rotating speed of 800r/min.
(3) irradiation complete after, centrifuged suspension, dried powder at 60 DEG C, obtain fullerene molybdenum disulfide microsphere.Products obtained therefrom pattern is similar to Example 1.
Embodiment 4
(1) weigh the original molybdenum disulphide powder of 5mg (purity 98%, granularity 200nm) in 100mL beaker, add 50mL dimethylformamide, ultrasonic disperse 20min, form suspension.
(2) suspension that will be prepared by krypton fluorine laser bundle (248nm) irradiation above-mentioned steps (1) after illuminator and convex lens focus, the molybdenum disulfide powder in ablation solvent, laser energy density 1200mJpulse-1cm-1, frequency 10Hz, laser pulse 40ns, exposure time is 10min.In laser beam irradiation process, the container filling suspension is placed in mixture of ice and water and keeps low temperature, and be stirred continuously suspension with magnetic stirrer with the rotating speed of 400r/min.
(3) irradiation complete after, centrifuged suspension, dried powder at 60 DEG C, obtain fullerene molybdenum disulfide microsphere.Products obtained therefrom pattern is similar to Example 1.
Embodiment 5
The method adopting embodiment 4 prepares the mos2 microsphere of similar Fuller olefin structure, the difference is that: energy density is 500mJpulse-1cm-1, exposure time is 60min.
Comparative example 1
(1) weigh the original molybdenum disulphide powder of 2500mg (purity 98%, granularity 400nm) in 100mL beaker, add 50mL water or acetone, ultrasonic disperse 10min, form suspension.
According to the method for embodiment 1, suspension is carried out irradiation, after irradiation terminates, centrifugal, separation, remove solvent, gained powder is dry at 60 DEG C, obtains product.
Products obtained therefrom is more serious through the test display molybdenum disulfide powder adhesion of surface sweeping Electronic Speculum, it is difficult to spheroidization, as shown in Figure 4.It can thus be seen that product pattern is formed with certain impact by the change of solvent and molybdenum bisuphide concentration.
Comparative example 2
The method adopting embodiment 5 prepares the mos2 microsphere of similar Fuller olefin structure, the difference is that: in irradiation process, the container filling suspension is placed at normal temperatures, does not carry out low temperature ice bath process.After irradiation terminates, centrifugal, separation, remove solvent, gained powder is dry at 60 DEG C, obtains product.Products obtained therefrom there occurs annexation between surface sweeping Electronic Speculum test display molybdenum disulfide particles, and granule sphericity is poor, as shown in Figure 5.
In order to verify the antifriction performance of products obtained therefrom, carry out following experiment.
1, the various embodiments described above and comparative example being prepared product and be respectively added in saxol, carry out frictional behaviour test, addition is the 0.15wt% of liquid paraffin oil quality.Meanwhile, being also respectively added in saxol by the molybdenum disulphide powder powder stock prepared used by these products, carry out frictional behaviour test, addition is also 0.15wt%, as a comparison.
2, frictional behaviour method of testing: four-ball friction and wear is tested, meanwhile, with paraffin refined wax oil for blank.
3, result
The frictional property test result of each embodiment and comparative example product, is shown in table 1 below.
Table 1
It can thus be seen that the fullerene molybdenum disulphide microspheres product that the inventive method prepares has had good lifting on antifriction performance, hence it is evident that higher than comparative example product.The condition on production performances such as solvent species, raw material concentration in a solvent, the suspension temperature when irradiation have considerable influence.
Claims (9)
1. a laser fast preparation method for inorganic fullerene molybdenum disulfide microsphere, is characterized in that comprising the following steps:
(1) molybdenum disulfide powder is disperseed in organic solvent, form suspension；
(2) with the above-mentioned suspension of pulse laser irradiation, molybdenum disulfide powder is made to be changed into similar Fuller olefin structure under the effect of organic solvent and pulse laser；
(3) irradiation complete after, by centrifugal for suspension, separate, gained precipitation is dry, obtains the mos2 microsphere with similar Fuller olefin structure.
2. preparation method according to claim 1, is characterized in that: in step (1), and described organic solvent is dimethylformamide.
3. preparation method according to claim 1 and 2, is characterized in that: in step (1), and molybdenum disulfide powder concentration in organic solvent is 0.1～15mg/mL.
4. preparation method according to claim 1 and 2, is characterized in that: in step (2), and wavelength is 193nm～1534nm, and frequency is 5～10Hz, and pulse width is 1～50ns, and energy density is 500～1800mJpulse-1cm-2, exposure time is 5～600min.
5. preparation method according to claim 1 and 2, is characterized in that: in step (2), in pulse laser irradiation process, and the temperature controlling suspension is 0 DEG C～5 DEG C.
6. preparation method according to claim 1 and 2, is characterized in that: in step (2), suspension is stirred pulse laser irradiation, and mixing speed is 100～1500r/min.
7. preparation method according to claim 1 and 2, is characterized in that: in step (1), molybdenum disulfide powder purity is more than 90%.
8. preparation method according to claim 1 and 2, is characterized in that: in step (1), molybdenum disulfide powder granularity is at below 1um.
9. preparation method according to claim 1 and 2, is characterized in that: in step (3), baking temperature is lower than organic solvent boiling point.
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| CN106398802A (en) * | 2016-09-07 | 2017-02-15 | 济南大学 | Rapid laser preparing method for composite with graphene loaded with spherical inorganic fullerene molybdenum disulfide |
| CN108405871A (en) * | 2018-04-13 | 2018-08-17 | 济南大学 | It is a kind of that the method for sub-micron metal ball particle and its application in lubricating oil are prepared based on laser ablation method |
| CN111689518A (en) * | 2020-06-03 | 2020-09-22 | 中国科学技术大学 | Two-dimensional transition metal disulfide layer number controllable preparation and patterning preparation method based on surface plasma wave |
| CN112479257A (en) * | 2020-11-25 | 2021-03-12 | 华中科技大学 | Laser-induced chemical synthesis of micro-nano-scale MoS at normal atmospheric temperature2Method and application of |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106398802A (en) * | 2016-09-07 | 2017-02-15 | 济南大学 | Rapid laser preparing method for composite with graphene loaded with spherical inorganic fullerene molybdenum disulfide |
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| CN111689518A (en) * | 2020-06-03 | 2020-09-22 | 中国科学技术大学 | Two-dimensional transition metal disulfide layer number controllable preparation and patterning preparation method based on surface plasma wave |
| CN111689518B (en) * | 2020-06-03 | 2021-04-23 | 中国科学技术大学 | Two-dimensional transition metal disulfide layer number controllable preparation and patterning preparation method based on surface plasma wave |
| CN112479257A (en) * | 2020-11-25 | 2021-03-12 | 华中科技大学 | Laser-induced chemical synthesis of micro-nano-scale MoS at normal atmospheric temperature2Method and application of |
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